CN104538633B - Lithium ion battery electrode material and preparation method thereof - Google Patents
Lithium ion battery electrode material and preparation method thereof Download PDFInfo
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- CN104538633B CN104538633B CN201410770614.8A CN201410770614A CN104538633B CN 104538633 B CN104538633 B CN 104538633B CN 201410770614 A CN201410770614 A CN 201410770614A CN 104538633 B CN104538633 B CN 104538633B
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- lithium ion
- electrode material
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 21
- 239000007772 electrode material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 150000003752 zinc compounds Chemical class 0.000 claims abstract description 29
- 239000011701 zinc Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 6
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims abstract description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 30
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 14
- 125000004429 atom Chemical group 0.000 claims description 12
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 12
- 150000003217 pyrazoles Chemical class 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052725 zinc Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 2
- 238000010583 slow cooling Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052744 lithium Inorganic materials 0.000 abstract description 3
- 125000003226 pyrazolyl group Chemical group 0.000 abstract description 3
- 239000003446 ligand Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract 1
- 238000013508 migration Methods 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 10
- 239000012621 metal-organic framework Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000012937 correction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/06—Zinc compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to field of lithium ion battery, particularly to a kind of lithium ion battery electrode material and preparation method thereof.A kind of lithium ion battery electrode material, this electrode material is zinc compound, and chemical formula is C18H18N4O4Zn, wherein zinc compound is rhombic system,PbanSpace group, cell parameter isa=11.937 (8),b=8.935 (2),c=19.074 (2),α=β=γ=90, V=2034.5 (7)3.The zinc compound synthetic method of the present invention is simple, and the Stability Analysis of Structures that selected mixed ligand obtains, when it is as electrode material of lithium battery, in charge and discharge process, it mainly utilizes the atom N on pyrazole ring to carry out the migration of lithium ion for it, so its Stability Analysis of Structures, do not cave in during discharge and recharge.
Description
Technical field
The present invention relates to field of lithium ion battery, particularly to a kind of lithium ion battery electrode material and preparation method thereof.
Background technology
Metal organic framework compound receives extensively due to its variable chemical constitution, excellent character as porous material
General concern.By reasonably design, metal organic framework compound can be widely used in gas storage, lithium ion stores,
Catalytic field.But, the chemical stability of metal organic framework compound often limits its application in practice, many gold
Belong to organic frame compound the most easily decompose or cave in.If in more complicated cases, such as, when
It is as the electrode material of lithium ion battery, owing to the situation of electrolyte is increasingly complex, and this metal organic framework compound steady
Qualitative worse.
Summary of the invention
The technical problem to be solved is to provide a kind of lithium ion based on metal organic framework compound
Battery electrode material.
Further object is that the preparation method that above-mentioned lithium ion battery electrode material is provided.
A kind of lithium ion battery electrode material, this electrode material is zinc compound, and chemical formula is C18H18N4O4Zn, wherein
Zinc compound is rhombic system, Pban space group, and cell parameter is a=11.937 (8), b=8.935 (2), c=19.074
(2), α=β=γ=90, V=2034.5 (7)3。
The preparation method of above-mentioned lithium ion battery electrode material is: by organic compound 3,3 ', 5,5 '-tetramethyl-4,4 '-
Connection pyrazoles, M-phthalic acid, zinc oxide add to the mixed solvent of acetonitrile and water, are stirred at room temperature formation mixed liquor a,
Then by described mixed liquor a under the conditions of solvent thermal after reacting by heating slow cooling obtain mixed liquor b；Finally mixed liquor b is existed
7 days described zinc compounds derived above of left at room temperature.
Further, described heating-up temperature is 140 DEG C ~ 160 DEG C, and the reacting by heating time is 24 ~ 48 hours.
Further, described cooling is 2 DEG C/h ~ 5 DEG C/h and is down to room temperature.
Further, described 3,3 ', 5,5 '-tetramethyl-4,4 '-connection pyrazoles, M-phthalic acid, the mol ratio of zinc oxide are
1:1:1。
Further, the volume ratio of described acetonitrile and water is 1:2.
The application in lithium ion battery of the above-mentioned zinc compound.
There is advantages that
The zinc compound synthetic method of the present invention is simple, and the Stability Analysis of Structures that selected mixed ligand obtains, when it
During as electrode material of lithium battery, in charge and discharge process, it mainly utilizes the atom N on pyrazole ring to carry out lithium ion for it
Migrate, so its Stability Analysis of Structures, do not cave in during discharge and recharge.
Accompanying drawing explanation
Fig. 1 is the zinc compound coordination environment figure with metal center Zn of the present invention.
Fig. 2 is the structural representation of the zinc compound of the present invention.
Fig. 3 is the zinc compound of present invention thermogravimetric curve figure under air atmosphere.
Fig. 4 is that the zinc compound of the present invention is when the cycle performance figure that electric current density is 100mA/g.
Fig. 5 is the zinc compound of present invention high rate performance figure under different electric current densities.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It it not limitation of the invention.
Embodiment 1
By 0.2 mmol3,3 ', 5,5 '-tetramethyl-4,4 '-connection pyrazoles, 0.2 mmol M-phthalic acid and, 0.2 mmol
Zinc oxide adds to the mixed solvent of 15mL acetonitrile and water (wherein the volume ratio of acetonitrile and water is 1:2), at room temperature stirs
Mix formation mixed liquor a, then described mixed liquor a is inserted in 25mL reactor reacting by heating 36 under the conditions of solvent thermal 150 DEG C
It is down to room temperature with 3 DEG C/h after hour and obtains mixed liquor b, finally mixed liquor b is at room temperature stood 10 days and obtain described containing zinc
Compound, productivity is 58.6% (based on Zn).
Then above-claimed cpd is carried out structural characterization.
The X ray diffracting data of this compound is to visit on diffractometer in Bruker Smart Apex CCD face, uses MoKαSpoke
Penetrating (λ=0.71073), collect and carry out Lp factor correction with ω scan mode, absorption correction uses SADABS program.With
Direct method solution structure, then obtains whole non-hydrogen atom coordinate by difference Fourier method, and obtains hydrogen atom with theoretical hydrogenation method
Position (C H 1.083), is modified structure with method of least square.Evaluation work uses SHELXTL program bag on PC
Complete.Compound crystal parameter is shown in Table 1.Structure is shown in Fig. 1, Fig. 2.
Table 1. crystallographic parameter and structure elucidation
From the point of view of crystal structure, this compound belongs to rhombic system, and Pban space group, containing one in this asymmetric cell
Zn atom, half 3,3 ', 5,5 '-tetramethyl-4,4 '-connection pyrazoles molecule and half M-phthalic acid molecule, as shown in Figure 1.Its
In, Zn atom takes the 6 octahedral patterns of coordination, wherein Zn atom and 2 different 3,3 ', 5,5 '-tetramethyl-4,4 '-connection
Atom N coordination on pyrazoles molecule；And the oxygen atom on M-phthalic acid takes pattern and the Zn Atomic coordinate of double coordination；?
Eventually, under the interconnection function of M-phthalic acid, define a kind of one-dimensional chain structure as shown in Figure 2, and on pyrazole ring, another does not has
The atom N having coordination is then distributed in one-dimensional chain both sides, the beneficially absorption of lithium ion.
Fig. 3 is that the zinc compound of the present invention is risen to 900 DEG C by room temperature with the speed of 10 DEG C/min in air atmosphere
Thermogravimetric curve figure, as can be seen from the figure this zinc compound does not has any obvious change from room temperature to 380 DEG C, until
400 DEG C degrees Celsius just start to decompose, and therefore, the zinc compound of the present invention has good stability.
Embodiment 2
By 0.2 mmol3,3 ', 5,5 '-tetramethyl-4,4 '-connection pyrazoles, 0.2 mmol M-phthalic acid and, 0.2 mmol
Zinc oxide adds to the mixed solvent of 15mL acetonitrile and water (wherein the volume ratio of acetonitrile and water is 1:2), at room temperature stirs
Mix formation mixed liquor a, then described mixed liquor a is inserted in 25mL reactor reacting by heating 48 under the conditions of solvent thermal 140 DEG C
It is down to room temperature with 5 DEG C/h after hour and obtains mixed liquor b, finally mixed liquor b is at room temperature stood 7 days and obtain described containing zinc
Compound, productivity is 45.9% (based on Zn).
Embodiment 3
By 0.2 mmol3,3 ', 5,5 '-tetramethyl-4,4 '-connection pyrazoles, 0.2 mmol M-phthalic acid and, 0.2 mmol
Zinc oxide adds to the mixed solvent of 15mL acetonitrile and water (wherein the volume ratio of acetonitrile and water is 1:2), at room temperature stirs
Mix formation mixed liquor a, then described mixed liquor a is inserted in 25mL reactor reacting by heating 24 under the conditions of solvent thermal 160 DEG C
It is down to room temperature with 2 DEG C/h after hour and obtains mixed liquor b, finally mixed liquor b is at room temperature stood 8 days and obtain described containing zinc
Compound, productivity is 52.6% (based on Zn).
Embodiment 4
Then using above-mentioned zinc compound pulverize after as electrode material, the electrochemical property test of electrode material be by material
Material is assembled into button cell (CR-2032) in the glove box of full Ar to be carried out, by active substance, acetylene black and carboxymethyl cellulose
Element sodium is dissolved in furnishing mixed slurry in water according to the ratio that mass ratio is 7:2:1 and is coated with on Copper Foil, is dried 12h, punching at 80 DEG C of vacuum
Sheet can be prepared by electrode slice.With metal lithium sheet for electrode, 1MLiPF in battery assembling6Be dissolved in EC/DEC (volume ratio is 1:
1) solution is electrolyte, and Celgard 2300 is barrier film, is made into CR-2032 button cell in glove box.Battery is surveyed
12 h need to be stood in room temperature before examination.Charge and discharge cycles test uses LANDCT-2001A battery test system, at voltage under room temperature
Scope is to test under 0.1-3.0 V.
Fig. 4 is the zinc compound of the present invention under the 100 mA/g cycle performance figure of first 150 times, from figure, we are permissible
Finding out, this zinc compound first circle specific discharge capacity is 248mAh/g, and in ensuing circulation, this zinc compound is always
Remain good cyclical stability, specific discharge capacity is always stable at about 152mAh/g, and this is likely due at this containing zinc
In compound, the atom N on its special one-dimensional chain structure, the absorption of beneficially Li and desorption, therefore, this zinc compound
There is good cycle performance.
Fig. 5 is the high rate performance figure of zinc compound, when electric current density is from 50 to 100, during 200,400 mA/g, and electric discharge ratio
Capacity is distributed as 170,150,125,90 mAh/g, and when electric current density returns to 50 mA/g, the capacity of battery remains to return to
170 mAh/g, these results fully show that this zinc compound has excellent high rate performance.
Embodiment described above only have expressed embodiments of the present invention, and it describes more concrete and detailed, but can not
Therefore the restriction to the scope of the claims of the present invention it is interpreted as, as long as using the skill that the form of equivalent or equivalent transformation is obtained
Art scheme, all should fall within the scope and spirit of the invention.
Claims (3)
1. a lithium ion battery electrode material, it is characterised in that: this electrode material is zinc compound, and chemical formula is
C18H18N4O4Zn, this zinc compound is rhombic system, Pban space group, and cell parameter is a=11.937 (8), b=8.935
(2), c=19.074 (2), α=β=γ=90, V=2034.5 (7)3；Described structure cell is asymmetric cell, and this is asymmetric
Unit divides containing Zn atom, half 3,3 ', 5,5 '-tetramethyl-4,4 '-connection pyrazoles molecule and half M-phthalic acid
Son；Wherein, Zn atom takes the 6 octahedral patterns of coordination, wherein Zn atom and 2 different 3,3 ', 5,5 '-tetramethyl-4,
Atom N coordination on 4 '-connection pyrazoles molecule；And the oxygen atom on M-phthalic acid takes the pattern of double coordination and Zn atom to join
Position；Its chemical constitution is as follows:
。
2. the method preparing lithium ion battery electrode material as claimed in claim 1, it is characterised in that: by organic compound
Thing 3,3 ', 5,5 '-tetramethyl-4, in the middle of 4 '-connection pyrazoles, M-phthalic acid, zinc oxide addition to the mixed solvent of acetonitrile and water,
Be stirred at room temperature formation mixed liquor a, then by described mixed liquor a under the conditions of solvent thermal after reacting by heating slow cooling obtain
Mixed liquor b；Finally mixed liquor b is at room temperature stood 7 days described zinc compounds derived above；
Described heating-up temperature is 140 DEG C ~ 160 DEG C, and the reacting by heating time is 24 ~ 48 hours；
Described cooling is 2 DEG C/h ~ 5 DEG C/h and is down to room temperature；
Described 3,3 ', 5,5 '-tetramethyl-4,4 '-connection pyrazoles, M-phthalic acid, the mol ratio of zinc oxide be 1:1:1；
The volume ratio of described acetonitrile and water is 1:2.
3. a lithium ion battery electrode material as claimed in claim 1 application in lithium ion battery.
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| CN201410770614.8A CN104538633B (en) | 2014-12-15 | 2014-12-15 | Lithium ion battery electrode material and preparation method thereof |
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| CN201410770614.8A CN104538633B (en) | 2014-12-15 | 2014-12-15 | Lithium ion battery electrode material and preparation method thereof |
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| CN104538633B true CN104538633B (en) | 2016-11-16 |
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| CN105154980B (en) * | 2015-06-19 | 2017-08-11 | 福州大学 | A kind of anode material of lithium battery and preparation method thereof |
| CN106356531A (en) * | 2015-07-13 | 2017-01-25 | 华东师范大学 | Cobalt and zinc binary metal coordination polymer, preparation method thereof, application of cobalt and zinc binary metal coordination polymer serving as lithium battery anode material |
| CN105633455A (en) * | 2016-04-04 | 2016-06-01 | 陈锦 | Lithium ion battery electrode material and preparation method thereof |
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| JP2002216764A (en) * | 2001-01-22 | 2002-08-02 | Junko Shigehara | Positive electrode material, lithium secondary battery and lithium ion secondary battery using the same |
| JP4314508B2 (en) * | 2002-04-15 | 2009-08-19 | 日本電気株式会社 | Radical battery |
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